Method for direct determination of titanium carbide content in titanium carbide slag by X-ray fluorescence spectrometry

A technology of ray fluorescence spectroscopy and fluorescence spectroscopy, which is applied in the field of physical and chemical detection, can solve the problems of large influence of human factors, large fluctuations in results, and inability to meet, and achieve stable and reliable results.

Active Publication Date: 2019-10-08
PANGANG GRP PANZHIHUA STEEL & VANADIUM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Titanium in titanium carbide slag is TiC, Ti n o m At present, the analysis techniques of titanium carbide in titanium carbide slag include: one is to measure the total titanium and low-valent titanium by photometry, and then calculate the content of titanium carbide by subtraction; the other is to separate titanium carbide from sulfuric acid-hydrofluoric acid. Titanium carbide is determined by spectrophotometry after nitric acid is dissolved. The method is manual analysis, which is greatly influenced by human factors, resulting in large fluctuations in results. The detection cycle is more than 4 hours, which cannot meet the requirements of on-site large-scale industrial production process control.

Method used

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  • Method for direct determination of titanium carbide content in titanium carbide slag by X-ray fluorescence spectrometry
  • Method for direct determination of titanium carbide content in titanium carbide slag by X-ray fluorescence spectrometry
  • Method for direct determination of titanium carbide content in titanium carbide slag by X-ray fluorescence spectrometry

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Experimental program
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Effect test

Embodiment 1

[0050] Embodiment 1 X-ray fluorescence spectrometry directly measures the method for titanium carbide content in titanium carbide slag

[0051] (1) Preparation of sample (A# sample)

[0052] a Titanium carbide phase separation

[0053] Accurately weigh 0.2000g titanium carbide slag sample, add 19wt% hydrochloric acid 50mL (19wt% hydrochloric acid is used density is 1.179g / cm 3 , concentrated hydrochloric acid with a mass fraction of 36% and water at a volume ratio of 1:1), 63wt% sulfuric acid 10mL (63wt% sulfuric acid is prepared with a density of 1.84g / cm 3 , with a mass fraction of 98% concentrated sulfuric acid and water in a volume ratio of 1:1), 40wt% concentrated hydrofluoric acid 3mL, heated to boiling at low temperature, and kept boiling slightly for 22min. Cool, filter with ash-free filter paper in a 500mL Erlenmeyer flask, and wash the residue.

[0054] b residue burning

[0055] Put the washed residue together with the filter paper in a platinum yellow crucible,...

Embodiment 2

[0076] Embodiment 2 accuracy test

[0077] Since there is no standard sample for carbide slag at present, we use standard sample preparation and comparison to test the accuracy of the method.

[0078] (1) Take 4 parts of 0.1500g vanadium-titanium blast furnace slag standard sample (YSBC19815-2014), then weigh 21.1mg, 25.2mg, 30.2mg of 99% titanium carbide respectively, test the three samples according to the method of the present invention, test The results are shown in Table 2, and the test values ​​are consistent with the theoretical values.

[0079] Table 2

[0080] serial number TiC addition amount mg Theoretical value% test value% 0 0 0 0 1 21.1 10.55 10.57 2 25.2 12.60 12.65 3 30.2 15.10 15.17

[0081] (2) Get 10 titanium carbide samples, adopt this method and chemical method (photometric method) to carry out comparison test, titanium carbide test result is as table 3, shows with paired data t test, two kinds of methods h...

Embodiment 3

[0084] Embodiment 3 precision test

[0085] In order to verify the precision of this method, the A# and B# samples were tested 10 times (Table 4, Table 5). The stability and good reproducibility of the method were examined from the precision of the experimental data. The relative standard deviations of Table 4 and Table 5 are all within a small range, indicating that the entire operation process of the method is stable and reliable.

[0086] Table 4

[0087]

[0088] table 5

[0089]

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Abstract

The invention relates to a method for measuring the content of titanium carbide in titanium carbide slag by the aid of X-ray fluorescent spectrometry, and belongs to the technical field of physical and chemical detection. The method includes dissolving the titanium carbide slag by the aid of hydrochloric acid-sulfuric acid-hydrofluoric acid to separate the titanium carbide from different types of titanium oxide; separating test specimens and then burning and melting residues to obtain sheets; plotting calibration curves by the aid of standard titanium dioxide; measuring the content of titanium in the titanium carbide by the aid of the X-ray fluorescent spectrometry. The method has the advantages of high speed and efficiency, low cost, safety and environmental protection. Besides, the method is quite suitable for quick on-the-spot sample analysis.

Description

technical field [0001] The invention relates to a method for directly measuring the content of titanium carbide in titanium carbide slag by X-ray fluorescence spectrometry, belonging to the technical field of physical and chemical detection. Background technique [0002] Panzhihua Iron and Steel Blast Furnace Titanium Slag is a unique titanium resource in my country, and its comprehensive utilization has always been one of the country's most difficult problems. Panzhihua Iron and Steel Co., Ltd. adopts the process route of "high-temperature carbonization-low temperature selective chlorination" for high-titanium blast furnace slag to carry out industrial tests on the high-temperature carbonization pilot line. During the production process of the carbonization process, the level of titanium carbide in the carbide slag is the key to guide the process control. For important parameters, there is an urgent need for fast, efficient and accurate analytical techniques for the determi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/223
Inventor 杨新能冯宗平李小青羊绍松
Owner PANGANG GRP PANZHIHUA STEEL & VANADIUM
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